绒螯蟹中3种氟喹诺酮类药物残留检测的前处理方法研究

Effects of Sample Pretreatment on Three Kinds of Quinolones Residues Determination in Fishery Products by High Performance Liquid Chromatography

研究了液相色谱法测定中华绒螯蟹组织中诺氟沙星、环丙沙星和恩诺沙星残留的前处理方法。结果表明：以提取前用无水硫酸钠作脱水剂、酸化乙腈作提取剂振荡提取、正已烷去脂、旋转蒸发并离心的前处理方法,灵敏、快速、准确、经济、实用性强。诺氟沙星、环丙沙星和恩诺沙星的最低检测限分别为5.0μg/kg、1.0μg/kg、5.0μg/kg;在加入标准品水平分别为5.0-15.0μg/kg、1.0-5.0μg/kg和5.0-15.0μg/kg时,回收率分别为68.67%-82.89%、66.67%-74.83%和72.67%-81.33%,相对标准偏差分别为1.22%-7.32%、5.19%-8.18%和2.52%-5.73%。该前处理方法适合检测诺氟沙星、环丙沙星和恩诺沙星残留。

The effects of sample pretreatments on norfloxacin, ciprofloxacin and enrofloxacin residues measurement in Eriocheir sinensis by high performance liquid chromatography was studied. The samples were dehydrated by sodium sulfate and the quinolones were abstracted in acid acetonitrile by gyratory shaker. The fat was extracted into hexane. The samples were concentrated by rotary evaporator. The other residues in the samples were removed by centrifuging. The method was proved to be sensitive, rapid, precise, economical and applied. The minimum detectable amount of norfloxacin, ciprofloxacin and enrofloxacin were 5. 0 μg/kg, 1.0 μg/kg and 5.0 μg/kg respectively. The averaged recoveries ranged from 68. 67%-82. 89%,66. 67%-74. 83% and 72. 67%-81. 33% at spiking levels of 5. 0-15. 0 μg/kg,1.0-5.0 μg/kg and 5. 0-15.0 μg/kg. The relative standard deviation were 1.22%-7.32%, 5.19%-8. 18% and 2. 52%-5. 73% respectively. It is suitable to measure the residues of norfloxacin, ciprofloxacin and enrofloxacin.